A Rapid and reliable thin-layer chromatographic method for the simultaneous estimation of celecoxib and diacerein in the
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INAL RESEARCH PAPER
A Rapid and reliable thin‑layer chromatographic method for the simultaneous estimation of celecoxib and diacerein in their binary mixture using nanosilica gel plate Mohamed Mohamed Salem Rizk1 · Safaa Shafik Toubar1 · Emad Ramzy Abd almalak Gadallah1 · Marwa Ibrahim Mohamed Helmy1 Received: 4 August 2020 / Accepted: 22 October 2020 / Published online: 20 November 2020 © Akadémiai Kiadó, Budapest, Hungary 2020
Abstract A novel, rapid, and sensitive stability-indicating high-performance thin-layer chromatography method was developed and validated for the simultaneous determination of celecoxib (CEL) and diacerein (DIA) in bulk and a capsule binary mixture. The complete separation was achieved by the proposed method on nanosilica gel F254 plates using n-hexane‒ethyl acetate‒ tetrahydrofuran‒glacial acetic acid (7:3:1:0.8, V/V) as the mobile phase. The chromatographic bands were visualized using short-wave ultraviolet light, and the amount of CEL and DIA was determined by scanning densitometry at 254 nm using the peak area. The RF values were 0.59 and 0.37 for CEL and DIA, respectively. From regression plots, it was found that good linearity was achieved in the concentration ranges of 20.00–320.00 ng/band and 5.00–80.00 ng/band with mean percentage recoveries 99.86 ± 0.70 and 99.64 ± 0.96 for CEL and DIA, respectively. The proposed method was validated according to the International Conference on Harmonisation guidelines. The statistical analysis of the results revealed high accuracy and precision, the suggested procedures could be used as a stability-indicating assay for the simultaneous determination of CEL and DIA in bulk drug and their capsule binary mixture in the presence of their degradation products. Keywords Celecoxib · Diacerein · Stability-indicating · HPTLC · Nanoplate Abbreviations CEL Celecoxib DIA Diacerein THF Tetrahydrofuran SD Standard deviation RSD Relative standard deviation SE Standard error Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00764-020-00064-7) contains supplementary material, which is available to authorized users. * Marwa Ibrahim Mohamed Helmy [email protected] Mohamed Mohamed Salem Rizk [email protected] Safaa Shafik Toubar [email protected] Emad Ramzy Abd almalak Gadallah [email protected] 1
Analytical Chemistry Department, Faculty of Pharmacy, Helwan University, Ein Helwan, Cairo 11795, Egypt
RF Retention factor LOQ Limit of quantification LOD Limit of detection
1 Introduction Celecoxib (CEL) (Fig. 1a) is a nonsteroidal antiinflammatory drug (NSAID) chemically designated as 4-[5-(4-methylphenyl)3-(trifluoromethyl)-1H-pyrazol1-yl]benzenesulfonamide, and it is an official drug in the British Pharmacopoeia (BP) [1] and the United States Pharmacopeia (USP) [2]. It is effectively utilized in the management of pain and inflammation. It has a great advantage over known traditional NSAIDs as (CEL) is a COX-2 specific inhibitor promoting suppression of the inflamm
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